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Method for extracting sulfur and inorganic salt from wet-desulfurization waste sulfur paste

A sulfur paste, sulfur technology, applied in chemical instruments and methods, thiosulfate/dithionite/polythionate, inorganic chemistry, etc., can solve the need for sewage discharge, large equipment investment, complex operation, etc. problem, to achieve the effect of strong fluctuation adaptability, high purity and high extraction yield

Active Publication Date: 2013-03-20
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the Chinese patent application No. 2007101395747 uses catalytic oxidation to desalinate waste liquid containing salt, but a new pollution source is introduced during the treatment process, and the sewage still needs to be discharged
More patents, such as patents with application numbers 200710044751, 201010173380, and 200610031074, all utilize the difference in the solubility of ammonium thiosulfate and ammonium thiocyanate with temperature, and adopt a crystallization process to separate the salt in the waste liquid. There are problems such as long process, complicated operation and large equipment investment in the process

Method used

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  • Method for extracting sulfur and inorganic salt from wet-desulfurization waste sulfur paste

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Effect test

Embodiment 1

[0020] A method for extracting sulfur and inorganic salts from wet desulfurization waste sulfur paste, comprising the steps of:

[0021] (1) Take 100g of powdered sulfur paste obtained by spray drying (containing about 24.8% sulfur, about 43.6% ammonium thiosulfate, about 31.6% ammonium thiocyanate) into a 500ml three-necked bottle, add methanol and acetone Mixed solution 100g (wherein the mass fraction of methanol is 85%, the mass fraction of acetone is 15%), stir at room temperature for 1h, filter and wash the filter cake with 20g of the above organic solvent, filter, the obtained filtrate is ammonium thiocyanate solution, filter cake It is a mixture of sulfur, ammonium thiosulfate and other insoluble impurities. After the filtrate is decolorized and distilled under reduced pressure, the temperature is controlled below 80°C, the distillation pressure is controlled below 10kPa (absolute pressure), and 100g of solvent is evaporated to obtain a concentrated solution. 98%, the ...

Embodiment 2

[0026] A method for extracting sulfur and inorganic salts from wet desulfurization waste sulfur paste, comprising the steps of:

[0027] (1) Take 200g of spray-dried powdered sulfur paste (containing about 22.5% sulfur, about 45.2% ammonium thiosulfate, and about 32.3% ammonium thiocyanate) into a 1000ml three-necked bottle, add 250g methanol, and stir at room temperature 45min, filter and wash the filter cake with 40g methanol, filter, the filtrate obtained is the methanol solution of ammonium thiocyanate, the filter cake is the mixture of sulfur, ammonium thiosulfate and other insoluble impurities, the filtrate is distilled under reduced pressure, and the temperature is controlled at 80 Below ℃, the distillation pressure is controlled below 10kPa (absolute pressure), and 200g of solvent is distilled to obtain a concentrated solution. The concentrated solution is cooled and crystallized, and 65.4g of ammonium thiocyanate crystals are obtained by filtration, with a content of 9...

Embodiment 3

[0031] A method for extracting sulfur and inorganic salts from wet desulfurization waste sulfur paste, comprising the steps of:

[0032] (1) Extract ammonium thiocyanate: Mix 100g of dried powdered sulfur paste with 90g of methanol and acetone mixed solution (85% by mass of methanol and 15% by mass of acetone), and stir at room temperature for 0.5 h, filter, wash the solid with 20g of the above solvent, filter to obtain the filtrate and filter cake, combine the filtrate, decolorize the filtrate, distill under reduced pressure below 80°C, distill 90 parts by mass of organic solvent to obtain a concentrated solution, and the concentrated solution crystallizes on cooling , filtered to obtain ammonium thiocyanate crystals (29.5g, content of 97.5%) and mother liquor, the mother liquor was reused in the crystallization process;

[0033] (2) Separation of sulfur and ammonium thiosulfate: dry the filter cake, mix with water equivalent to 90% of the mass of the filter cake, stir at roo...

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Abstract

The invention discloses a method for extracting sulfur and inorganic salt from wet-desulfurization waste sulfur paste, which comprises the following steps: (1) mixing powdery sulfur paste and an organic solvent, stirring, filtering, washing the solid with the organic solvent, filtering to obtain a filtrate and a filter cake, merging the filtrates, decolorizing, carrying out vacuum distillation to remove the organic solvent and obtain a concentrated solution, cooling the concentrated solution, crystallizing, and filtering to obtain ammonium thiocyanate crystals and a mother solution; (2) drying the filter cake, mixing with water, stirring at room temperature for 0.5-2 hours, filtering, washing with water, merging the filtrates, and drying the filter cake to obtain a sulfur product; and (3) carrying out vacuum distillation on the filtrate, cooling to crystallize, and filtering to obtain the ammonium thiosulfate crystals. The method disclosed by the invention has the advantages of simple technique, short process, stable operation and strong adaptability to raw material yield and component fluctuation; and by treating the desulfurization waste liquid in the wet-desulfurization production process, the invention reutilizes the waste and reduces the environmental pollution. The extraction yield is high, and the purities of the extracted ammonium thiocyanate, sulfur and ammonium thiosulfate are high.

Description

technical field [0001] The invention relates to a method for extracting sulfur and inorganic salts from wet desulfurization waste sulfur paste. Background technique [0002] my country is the world's largest coal producer and consumer, SO emissions in the atmosphere 2 90% of that comes from dry coal. It is essential for desulfurization and decyanation treatment of coal-fired flue gas and gas. At present, my country's coking plants and other coal-fired tail gas treatment mostly use HPF wet desulfurization process. This method has the advantages of low investment, high desulfurization efficiency, low operating cost, low energy consumption, and easy operation. It is widely used in the field of desulfurization . [0003] However, in the wet desulfurization process, it will inevitably be produced in the desulfurization liquid phase (NH 4 ) 2 S 2 o 3 , NH 4 Inorganic salts such as CNS, most of these salts are accumulated in desulfurization waste liquid. When the salt conte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/027C01B17/64C01C3/20
Inventor 范江洋陈松李国兵韩毅汤元睿
Owner TIANJIN UNIV
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